匹可硫酸钠的合成工艺改进

Improvement of Synthesis Technology for Sodium Picosulfate

目的:改进匹可硫酸钠的合成工艺。方法:通过改变反应溶剂、加料方式、精制方法和形成结晶水等方法对匹可硫酸钠的合成工艺进行改进。以苯酚为起始原料,与2-吡啶甲醛缩合制得4,4′-(吡啶-2-基亚甲基)双苯酚,并考察其收率;然后经酯化、成盐,形成结晶水得到匹可硫酸钠,再考察其纯度。结果:关键中间体4,4′-(吡啶-2-基亚甲基)双苯酚的收率达88%以上,精制后的产品纯度达99.5%以上。匹可硫酸钠一水合物稳定,单一杂质含量小于0.1%。结论:改进后的工艺简单、条件温和,适合大规模生产。

OBJECTIVE：To improve the synthesis technology of sodium picosulfate. METHODS：The synthesis technology of sodium picosulfate was improved by changing reaction solvent,charging sequence,refined method and formation of crystal water.Using phenol as raw material,it was condensed with 2-pyridinecarboxaldehyde to achieve 4,4′-（pyridin-2-ylmethylene）diphenol,and its yield rate was investigated. Sodium picosulfate was obtained after esterification,salification,formation of crystal water,and then its purity was determined. RESULTS：The yield rate of key intermediate 4,4′-（pyridin-2-ylmethylene）diphenol reached above 88%,and the purity of refined products reached over 99.5%. Sodium picosulfate monohydrate was stable,and the content of single impurity was less than 0.1%. CONCLUSIONS：The improved technology is simple with mild conditions,and suitable for large-scale production.